関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Pyrazole | HCID 1048 | — |
| 反応物 | Phenacyl bromide | HCID 6259 | — |
| 反応物 | Potassium Carbonate | HCID 11430 | — |
| 反応物 | HCID 178418231 | HCID 178418231 | — |
| 溶媒 | Acetone | HCID 180 | — |
| 生成物 | 4-Methoxyimino-5-methyl-6-(1-ethyl-5-phenacyloxypyrazol-4-yl)carbonylthiochroman-1,1-dioxide | HCID 86752170 | 52% |
反応手順
0.4 Gram (1.1 mmol) of 4-methoxyimino-5-methyl-6-(1-ethyl-5-hydroxypyrazol-4-yl)carbonylthiochroman-1,1-dioxide corresponding to pyrazole derivative (I-H), 0.23 g (1.2 mmol) of phenacyl bromide corresponding to compound B-A-Hal and 0.15 g of potassium carbonate were added to 10 ml of acetone, and the mixture was stirred under heat for 8 hours. Insolubles were removed by filtration, and then the acetone was distilled off. The residue was dissolved in ethyl acetate, and the mixture was washed with a saturated sodium chloride aqueous solution and dried over sodium sulfate. The ethyl acetate was distilled off under reduced pressure, and the residue was subjected to column chromatography (hexane/ethyl acetate) to give 4-methoxyimino-5-methyl-6-(1-ethyl-5-phenacyloxypyrazol-4-yl)carbonylthiochroman-1,1-dioxide (Compound Ib-2) at a yield of 52%.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US05723408 |
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| 出典データセット | uspto-grants-1998_03 |
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| ORD ID | ord-7676d3f705f64b5888f4950efb2b2f22 |
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| 出典メモ | uspto-grants-1998_03 |
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